#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322312.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4322312
loop_
_publ_author_name
'Isabel Castro'
'María Luisa Calatayud'
'Jorunn Sletten'
'Francesc Lloret'
'Juan Cano'
'Miguel Julve'
'Gunther Seitz'
'Klaus Mann'
_publ_section_title
;
 Ferro- and Antiferromagnetic Coupling through 1,n-Dithiosquarate Bridges
 (n= 2, 3) in Copper(II) Dimers. Syntheses, Crystal Structures, and
 Magnetic Properties of [Cu2(bpca)2(1,2-dtsq)(H2O)].2H2O and
 [Cu2(bpca)2(1,3-dtsq)].2H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4680
_journal_page_last               4687
_journal_paper_doi               10.1021/ic9904384
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_moiety         'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_structural     'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_sum            'C28 H22 Cu2 N6 O9 S2'
_chemical_formula_weight         777.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.276(2)
_cell_angle_beta                 100.009(2)
_cell_angle_gamma                94.139(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3243(4)
_cell_length_b                   10.9036(5)
_cell_length_c                   15.5432(4)
_cell_measurement_temperature    223(2)
_cell_volume                     1551.90(11)
_computing_cell_refinement       'SAINT, version 4.0'
_computing_data_collection       'SMART, version 4.0'
_computing_data_reduction        'SAINT, version 4.0'
_computing_molecular_graphics    XP-97
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       '2K Smart CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24800
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time
;
        50 first frames remeasured at end ofdata collection
;
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   'numerical integration'
_exptl_crystal_colour            'brownish green'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       no
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_obs          0.0662
_refine_ls_shift/esd_max         0.123
_refine_ls_shift/esd_mean        0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0820P)²+2.9629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1854
_refine_ls_wR_factor_obs         0.1612
_reflns_number_observed          5033
_reflns_number_total             7737
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9904384_1.cif
_cod_data_source_block           cu12dtsq
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+2.9629P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+2.9629P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322312
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu1 Cu 0.63954(7) 0.37071(6) 0.06771(4) 0.0492(2) Uani 1 d . .
Cu2 Cu 0.77138(6) 0.17031(5) 0.36886(4) 0.0376(2) Uani 1 d . .
S1 S 0.66804(14) 0.24593(12) 0.23451(8) 0.0419(3) Uani 1 d . .
S2 S 0.46617(13) 0.48474(12) 0.10851(8) 0.0427(3) Uani 1 d . .
O1 O 1.0430(6) 0.2831(7) 0.0420(5) 0.125(3) Uani 1 d . .
O2 O 0.8183(10) 0.1300(6) -0.0707(5) 0.154(4) Uani 1 d . .
O3 O 0.3715(5) 0.5801(4) 0.3089(3) 0.0608(10) Uani 1 d . .
O4 O 0.5487(5) 0.3615(4) 0.4210(2) 0.0605(10) Uani 1 d . .
O5 O 0.8314(5) -0.0531(4) 0.5772(3) 0.0600(11) Uani 1 d . .
O6 O 1.0343(5) 0.1586(4) 0.6052(2) 0.0642(11) Uani 1 d . .
O7 O 0.8978(4) 0.0463(4) 0.2872(2) 0.0587(10) Uani 1 d . .
O8 O 0.7768(11) -0.2190(7) 0.7153(5) 0.152(3) Uani 1 d . .
O91 O 1.1882(24) 0.0963(16) 0.1348(13) 0.094(6) Uani 0.30 d P .
O92 O 1.0501(11) 0.0621(8) 0.1381(5) 0.097(3) Uani 0.70 d P .
N1 N 0.8162(5) 0.4921(6) 0.1169(3) 0.065(2) Uani 1 d . .
N2 N 0.7907(6) 0.2891(6) 0.0248(4) 0.068(2) Uani 1 d . .
N3 N 0.5065(6) 0.2374(4) 0.0012(3) 0.0585(13) Uani 1 d . .
N4 N 0.6165(4) 0.0334(4) 0.3791(3) 0.0424(9) Uani 1 d . .
N5 N 0.8520(4) 0.1134(4) 0.4852(3) 0.0415(9) Uani 1 d . .
N6 N 0.9353(4) 0.3028(4) 0.4030(3) 0.0412(9) Uani 1 d . .
C1 C 0.8181(7) 0.5979(7) 0.1621(5) 0.069(2) Uani 1 d . .
H1 H 0.7299(7) 0.6260(7) 0.1730(5) 0.103 Uiso 1 calc R .
C2 C 0.9485(8) 0.6659(9) 0.1927(5) 0.094(3) Uani 1 d . .
H2 H 0.9460(8) 0.7406(9) 0.2227(5) 0.141 Uiso 1 calc R .
C3 C 1.0758(10) 0.6298(10) 0.1814(6) 0.098(3) Uani 1 d . .
H3 H 1.1629(10) 0.6770(10) 0.2036(6) 0.147 Uiso 1 calc R .
C4 C 1.0782(6) 0.5229(9) 0.1370(5) 0.080(3) Uani 1 d . .
H4 H 1.1673(6) 0.4949(9) 0.1275(5) 0.119 Uiso 1 calc R .
C5 C 0.9443(7) 0.4539(7) 0.1049(4) 0.067(2) Uani 1 d . .
C6 C 0.9327(7) 0.3363(8) 0.0543(5) 0.084(3) Uani 1 d . .
C7 C 0.7476(10) 0.1955(7) -0.0295(5) 0.082(2) Uani 1 d . .
C8 C 0.5836(11) 0.1658(6) -0.0444(4) 0.079(2) Uani 1 d . .
C9 C 0.5097(15) 0.0759(8) -0.0985(6) 0.106(3) Uani 1 d . .
H9 H 0.5624(15) 0.0261(8) -0.1294(6) 0.159 Uiso 1 calc R .
C10 C 0.3615(17) 0.0550(8) -0.1096(5) 0.119(4) Uani 1 d . .
H10 H 0.3127(17) -0.0058(8) -0.1494(5) 0.178 Uiso 1 calc R .
C11 C 0.2803(12) 0.1277(7) -0.0594(6) 0.101(3) Uani 1 d . .
H11 H 0.1786(12) 0.1140(7) -0.0636(6) 0.152 Uiso 1 calc R .
C12 C 0.3603(8) 0.2183(6) -0.0051(4) 0.070(2) Uani 1 d . .
H12 H 0.3117(8) 0.2679(6) 0.0284(4) 0.104 Uiso 1 calc R .
C13 C 0.5657(5) 0.3563(4) 0.2634(3) 0.0368(10) Uani 1 d . .
C14 C 0.4899(4) 0.4466(4) 0.2163(3) 0.0330(9) Uani 1 d . .
C15 C 0.4409(5) 0.4962(5) 0.2941(3) 0.0436(11) Uani 1 d . .
C16 C 0.5239(5) 0.3946(5) 0.3462(3) 0.0436(11) Uani 1 d . .
C17 C 0.4921(6) 0.0037(5) 0.3252(3) 0.0506(13) Uani 1 d . .
H17 H 0.4629(6) 0.0548(5) 0.2778(3) 0.076 Uiso 1 calc R .
C18 C 0.4033(7) -0.1012(6) 0.3368(4) 0.061(2) Uani 1 d . .
H18 H 0.3169(7) -0.1217(6) 0.2968(4) 0.091 Uiso 1 calc R .
C19 C 0.4437(8) -0.1742(5) 0.4073(4) 0.062(2) Uani 1 d . .
H19 H 0.3850(8) -0.2451(5) 0.4163(4) 0.093 Uiso 1 calc R .
C20 C 0.5711(7) -0.1424(5) 0.4648(4) 0.0543(14) Uani 1 d . .
H20 H 0.6009(7) -0.1910(5) 0.5136(4) 0.081 Uiso 1 calc R .
C21 C 0.6534(6) -0.0381(4) 0.4493(3) 0.0420(11) Uani 1 d . .
C22 C 0.7898(6) 0.0057(5) 0.5119(3) 0.0492(13) Uani 1 d . .
C23 C 0.9693(6) 0.1778(5) 0.5316(3) 0.0455(12) Uani 1 d . .
C24 C 1.0190(6) 0.2850(5) 0.4813(3) 0.0433(11) Uani 1 d . .
C25 C 1.1424(6) 0.3583(6) 0.5128(4) 0.0531(13) Uani 1 d . .
H25 H 1.1981(6) 0.3433(6) 0.5677(4) 0.080 Uiso 1 calc R .
C26 C 1.1841(7) 0.4548(6) 0.4631(4) 0.0607(15) Uani 1 d . .
H26 H 1.2694(7) 0.5056(6) 0.4828(4) 0.091 Uiso 1 calc R .
C27 C 1.0972(7) 0.4745(6) 0.3839(4) 0.0593(15) Uani 1 d . .
H27 H 1.1215(7) 0.5406(6) 0.3493(4) 0.089 Uiso 1 calc R .
C28 C 0.9757(6) 0.3979(5) 0.3560(3) 0.0496(12) Uani 1 d . .
H28 H 0.9180(6) 0.4122(5) 0.3016(3) 0.074 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N3 84.0(3) . . ?
N2 Cu1 N1 81.1(3) . . ?
N3 Cu1 N1 164.7(2) . . ?
N2 Cu1 S2 173.6(2) . . ?
N3 Cu1 S2 98.3(2) . . ?
N1 Cu1 S2 96.1(2) . . ?
N2 Cu1 S1 95.97(15) . . ?
N3 Cu1 S1 95.02(13) . . ?
N1 Cu1 S1 90.34(12) . . ?
S2 Cu1 S1 89.76(4) . . ?
N5 Cu2 N6 80.7(2) . . ?
N5 Cu2 N4 81.4(2) . . ?
N6 Cu2 N4 160.6(2) . . ?
N5 Cu2 S1 176.63(13) . . ?
N6 Cu2 S1 98.86(11) . . ?
N4 Cu2 S1 98.58(12) . . ?
N5 Cu2 O7 98.01(15) . . ?
N6 Cu2 O7 96.7(2) . . ?
N4 Cu2 O7 93.1(2) . . ?
S1 Cu2 O7 85.35(9) . . ?
C13 S1 Cu2 102.5(2) . . ?
C13 S1 Cu1 84.8(2) . . ?
Cu2 S1 Cu1 160.82(6) . . ?
C14 S2 Cu1 98.2(2) . . ?
C5 N1 C1 117.6(6) . . ?
C5 N1 Cu1 113.6(6) . . ?
C1 N1 Cu1 128.7(4) . . ?
C7 N2 C6 127.2(7) . . ?
C7 N2 Cu1 116.6(5) . . ?
C6 N2 Cu1 116.2(6) . . ?
C12 N3 C8 121.6(7) . . ?
C12 N3 Cu1 128.1(5) . . ?
C8 N3 Cu1 110.2(5) . . ?
C17 N4 C21 118.2(5) . . ?
C17 N4 Cu2 128.7(3) . . ?
C21 N4 Cu2 113.0(3) . . ?
C23 N5 C22 124.3(4) . . ?
C23 N5 Cu2 118.5(3) . . ?
C22 N5 Cu2 117.1(4) . . ?
C28 N6 C24 117.6(5) . . ?
C28 N6 Cu2 128.6(4) . . ?
C24 N6 Cu2 113.6(3) . . ?
N1 C1 C2 120.8(8) . . ?
N1 C1 H1 119.6(4) . . ?
C2 C1 H1 119.6(6) . . ?
C3 C2 C1 122.4(10) . . ?
C3 C2 H2 118.8(6) . . ?
C1 C2 H2 118.8(6) . . ?
C2 C3 C4 118.4(8) . . ?
C2 C3 H3 120.8(6) . . ?
C4 C3 H3 120.8(5) . . ?
C3 C4 C5 119.1(7) . . ?
C3 C4 H4 120.5(5) . . ?
C5 C4 H4 120.4(5) . . ?
N1 C5 C4 121.7(8) . . ?
N1 C5 C6 114.3(6) . . ?
C4 C5 C6 124.1(7) . . ?
O1 C6 N2 123.3(9) . . ?
O1 C6 C5 122.5(8) . . ?
N2 C6 C5 114.1(6) . . ?
O2 C7 N2 130.9(9) . . ?
O2 C7 C8 116.1(9) . . ?
N2 C7 C8 112.9(6) . . ?
C9 C8 N3 118.7(9) . . ?
C9 C8 C7 125.3(9) . . ?
N3 C8 C7 116.0(7) . . ?
C8 C9 C10 122.2(10) . . ?
C8 C9 H9 118.9(7) . . ?
C10 C9 H9 118.9(6) . . ?
C9 C10 C11 119.3(8) . . ?
C9 C10 H10 120.4(6) . . ?
C11 C10 H10 120.4(6) . . ?
C12 C11 C10 116.4(9) . . ?
C12 C11 H11 121.8(6) . . ?
C10 C11 H11 121.8(6) . . ?
N3 C12 C11 121.7(8) . . ?
N3 C12 H12 119.2(4) . . ?
C11 C12 H12 119.1(6) . . ?
C14 C13 C16 92.8(4) . . ?
C14 C13 S1 132.7(4) . . ?
C16 C13 S1 134.5(4) . . ?
C13 C14 C15 93.3(4) . . ?
C13 C14 S2 132.5(4) . . ?
C15 C14 S2 134.3(4) . . ?
O3 C15 C14 135.7(5) . . ?
O3 C15 C16 137.6(5) . . ?
C14 C15 C16 86.6(4) . . ?
O4 C16 C13 135.3(5) . . ?
O4 C16 C15 137.4(5) . . ?
C13 C16 C15 87.3(4) . . ?
N4 C17 C18 121.9(5) . . ?
N4 C17 H17 119.1(3) . . ?
C18 C17 H17 119.0(4) . . ?
C19 C18 C17 119.1(6) . . ?
C19 C18 H18 120.4(4) . . ?
C17 C18 H18 120.4(4) . . ?
C18 C19 C20 119.4(5) . . ?
C18 C19 H19 120.3(4) . . ?
C20 C19 H19 120.3(3) . . ?
C21 C20 C19 118.4(5) . . ?
C21 C20 H20 120.8(4) . . ?
C19 C20 H20 120.8(3) . . ?
N4 C21 C20 123.0(5) . . ?
N4 C21 C22 115.8(4) . . ?
C20 C21 C22 121.3(5) . . ?
O5 C22 N5 128.2(6) . . ?
O5 C22 C21 120.3(5) . . ?
N5 C22 C21 111.5(4) . . ?
O6 C23 N5 128.6(5) . . ?
O6 C23 C24 120.0(5) . . ?
N5 C23 C24 111.4(4) . . ?
N6 C24 C25 122.6(5) . . ?
N6 C24 C23 115.6(5) . . ?
C25 C24 C23 121.8(5) . . ?
C24 C25 C26 119.2(5) . . ?
C24 C25 H25 120.4(3) . . ?
C26 C25 H25 120.4(3) . . ?
C27 C26 C25 118.2(6) . . ?
C27 C26 H26 120.9(4) . . ?
C25 C26 H26 120.9(3) . . ?
C28 C27 C26 119.8(5) . . ?
C28 C27 H27 120.1(3) . . ?
C26 C27 H27 120.1(4) . . ?
N6 C28 C27 122.5(5) . . ?
N6 C28 H28 118.7(3) . . ?
C27 C28 H28 118.7(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.930(5) . ?
Cu1 N3 2.000(6) . ?
Cu1 N1 2.071(6) . ?
Cu1 S2 2.2804(13) . ?
Cu1 S1 2.9137(12) . ?
Cu2 N5 1.956(4) . ?
Cu2 N6 2.024(4) . ?
Cu2 N4 2.027(4) . ?
Cu2 S1 2.3240(12) . ?
Cu2 O7 2.359(4) . ?
S1 C13 1.694(5) . ?
S2 C14 1.709(4) . ?
O1 C6 1.259(8) . ?
O2 C7 1.251(9) . ?
O3 C15 1.201(6) . ?
O4 C16 1.208(6) . ?
O5 C22 1.224(6) . ?
O6 C23 1.225(6) . ?
N1 C5 1.335(8) . ?
N1 C1 1.345(9) . ?
N2 C7 1.315(11) . ?
N2 C6 1.384(10) . ?
N3 C12 1.350(9) . ?
N3 C8 1.372(9) . ?
N4 C17 1.327(7) . ?
N4 C21 1.354(6) . ?
N5 C23 1.349(7) . ?
N5 C22 1.370(7) . ?
N6 C28 1.341(6) . ?
N6 C24 1.350(6) . ?
C1 C2 1.386(10) . ?
C1 H1 0.94 . ?
C2 C3 1.317(13) . ?
C2 H2 0.94 . ?
C3 C4 1.355(13) . ?
C3 H3 0.94 . ?
C4 C5 1.421(10) . ?
C4 H4 0.94 . ?
C5 C6 1.488(12) . ?
C7 C8 1.517(12) . ?
C8 C9 1.355(13) . ?
C9 C10 1.37(2) . ?
C9 H9 0.94 . ?
C10 C11 1.45(2) . ?
C10 H10 0.94 . ?
C11 C12 1.383(10) . ?
C11 H11 0.94 . ?
C12 H12 0.94 . ?
C13 C14 1.390(6) . ?
C13 C16 1.475(7) . ?
C14 C15 1.478(7) . ?
C15 C16 1.547(7) . ?
C17 C18 1.394(8) . ?
C17 H17 0.94 . ?
C18 C19 1.373(9) . ?
C18 H18 0.94 . ?
C19 C20 1.378(9) . ?
C19 H19 0.94 . ?
C20 C21 1.371(7) . ?
C20 H20 0.94 . ?
C21 C22 1.507(8) . ?
C23 C24 1.500(7) . ?
C24 C25 1.367(8) . ?
C25 C26 1.381(9) . ?
C25 H25 0.94 . ?
C26 C27 1.378(8) . ?
C26 H26 0.94 . ?
C27 C28 1.364(8) . ?
C27 H27 0.94 . ?
C28 H28 0.94 . ?
